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A kind of preparation method and application of amino functionalized MCM molecular sieve

A technology of amino functionalization and molecular sieves, which is applied in the direction of separation methods, chemical instruments and methods, molecular sieves and base exchange compounds, etc., and can solve the problems of poor order and reduced order degree of functionalized materials

Active Publication Date: 2022-01-04
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the functionalized materials prepared by the co-condensation method usually have the disadvantage of poor order, and the order will decrease with the increase of the amount of organic groups introduced.

Method used

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  • A kind of preparation method and application of amino functionalized MCM molecular sieve
  • A kind of preparation method and application of amino functionalized MCM molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Under the condition of 30°C, 9.6g of cetyltrimethylammonium bromide (CTAB) and 85.5g of deionized water were successively added into the reactor, stirred evenly, and then slowly added dropwise with 11g of ethyl orthosilicate ( TEOS), finally add 10.6g NaOH to adjust the pH of the solution to be 11~13, and the molar ratio of the obtained reaction mixture is SiO 2 : 90H 2 O: 0.5R: 5OH - , the mixture was transferred to a crystallization kettle, heated to 110° C., and crystallized at a constant temperature for 72 hours. After the crystallization is complete, when the temperature drops to room temperature, the reacted mixture is separated, washed, and dried at 110°C to obtain the original powder of MCM-41 molecular sieve. Take 5 g of the obtained MCM-41 molecular sieve powder and 0.0193 mol (2.1 g) of trimethylchlorosilane and stir for 3 h at 40 ° C, then mix the product with 0.0587 mol (15 g) of 3-(phenylamino) propyl trimethyl Oxysilane and 15g of ethanol were mixed un...

Embodiment 2

[0035] The difference from Example 1 is that the feeding temperature is changed to 40°C, the stencil agent is changed to cetyltrimethylammonium chloride (CTAC), the dosage is 4.1g, the amount of water is changed to 46.1g, and the silicon source Change to sodium silicate, the dosage is 9.1g, the amount of NaOH is changed to 7.7g, the crystallization temperature is changed to 120°C, the crystallization time is changed to 80h, the drying temperature is changed to 120°C, and the passivating agent is changed to dimethyl di Chlorosilane, the dosage is changed to 0.0232mol (3g), the passivation temperature is changed to 30°C, the passivation time is changed to 2h, the amino modifier is changed to 3-aminopropyltriethoxysilane, and the dosage is changed to 0.0391mol ( 10g), the modification temperature was changed to 60°C, the modification time was changed to 5h, the amount of ethanol was changed to 10g, the extraction agent was changed to diethyl ether, the amount was changed to 15g, t...

Embodiment 3

[0038] The difference from Example 1 is that the feeding temperature is changed to 50°C, the template agent is changed to cetyltrimethylammonium chloride (CTAC), the dosage is 3g, the amount of water is changed to 56.1g, and the amount of TEOS Changed to 6.5g, the alkali source was changed to ammonia water, the dosage was 4.4g, the crystallization temperature was changed to 130°C, the crystallization time was changed to 90h, the drying temperature was changed to 130°C, the passivating agent was changed to diphenyldichlorosilane, The dosage is changed to 0.0049mol (1.25g), the passivation temperature is changed to 60°C, the passivation time is changed to 6h, the amino modifier is changed to 3-aminopropyltrimethoxysilane, and the dosage is changed to 0.0557mol (10g), The modification temperature was changed to 90°C, the modification time was changed to 6h, the amount of ethanol was changed to 10g, the extraction agent was changed to diethyl ether, the dosage was changed to 10g, t...

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Abstract

The present invention relates to a preparation method of amino-functionalized MCM mesoporous molecular sieve, comprising the following steps: S1. Provide the original powder of MCM molecular sieve; preferably, mix organic template agent, water, silicon source and alkali source into gel, and gel The mixture is subjected to hydrothermal crystallization, followed by solid-liquid separation, and the separated solid phase is washed and dried to provide the MCM molecular sieve raw powder; S2. Mix the MCM mesoporous molecular sieve raw powder with a passivating agent for Passivate, then mix and react with an amino modifier, then separate the product from solid to liquid, and wash and dry the separated solid sample; S3. Mix the dried product in step S2 with an extractant for extraction , and then remove the liquid phase, and dry the solid phase to obtain the amino functionalized MCM mesoporous molecular sieve. The method does not destroy the molecular sieve channel structure and crystallinity, but can also graft amino groups inside the molecular sieve channel.

Description

technical field [0001] The invention provides a method for preparing a modified molecular sieve, in particular to a method for preparing an amino functionalized MCM molecular sieve and its application. Background technique [0002] Molecular sieves from the MCM mesoporous family of molecular sieves have shown great interest due to their large specific surface area, pore volume, and uniform pore size. The emergence of MCM mesoporous materials not only broadens the application range of molecular sieves but also makes up for the defects of microporous materials. However, the performance brought by the ordered pore structure and high specific surface area cannot meet the requirements of specific conditions. For example, in catalytic applications, biomolecular reactions, and chromatographic applications, the activity of the inner and outer surfaces of mesoporous materials is still not high enough, and the inner and outer surfaces of MCM-41 mesoporous materials lack active groups...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/04C01B39/02B01J20/18B01J20/30B01D53/02
CPCC01B39/04C01B39/026B01J20/186B01D53/02C01P2002/72C01P2002/82C01P2006/12
Inventor 吴凯任行涛刘艳惠贾志光杨光
Owner CHINA PETROLEUM & CHEM CORP